[Objective] To establish a rapid method for ultra-high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS) detection of amphenicol antibiotic residues in milk. The method should be capable of simultaneously detecting chloramphenicol,thiamphenicol,florfenicol and its main metabolite,florfenicolamine,and should have a relatively low limit of detection(LOD). [Method] The milk was precipitated with trichloroacetic acid to remove proteins,extracted with ammoniated ethyl acetate,purified by MCX solid-phase extraction column,and re-solubilized in a methanol-water solution,separated on a Waters ACQUITY UPLC HSS T3 column(2.1 mm×100 mm,1.8 μm),and eluted with a gradient of 25% methanol(channel A)and 75% water[containing 100 μL of ammoniated methanol(5%)in 200 mL water,channel B]. Mass spectrometry analysis was performed using multiple reaction monitoring(MRM),and quantification was determined by external standard method. [Result] This method could complete the detection of 4 amphenicol compounds within 5 minutes. The recovery rates of the 4 amphenicol compounds at the added levels of 0.3,0.6,1.5 μg/kg was 77.3% to 106.4%,with the relative standard deviation ranging from 1.6% to 11.8%(n=6). The LOD of the method was 0.1 μg/kg and the limit of quantification(LOQ)was 0.3 μg/kg. [Conclusion] This method was comprehensive,rapid,highly accurate,highly sensitive and stable,making it suitable for the detection of four amphenicol antibiotic residues in milk.
CUI Ting
,
SONG Zhenjuan
,
LIANG Fengling
,
CUI Qiang
,
BAI Yang
,
GUO Bairu
,
ZHANG Hao
. A Rapid Method for Determination of Amphenicol Residues in Milk[J]. China Dairy, 2026
, 0(7)
: 119
-127
.
DOI: 10.12377/1671-4393.26.07.16
[1] 中国兽药典委员会.中华人民共和国兽药典[M].化学工业出版社,2020.
[2] 姚佳,王昕,张建新.免疫亲和柱-高效液相色谱法测定牛奶中氯霉素和玉米赤霉醇及其类似物[J].食品科学,2014,35(18):124-127.
[3] 彭涛,李淑娟,储晓刚,等.高效液相色谱-串联质谱法同时测定虾中氯霉素、甲砜霉素和氟甲砜霉素残留量[J].分析化学,2005,33(4):463-466.
[4] 仲伶俐,郭灵安,毛建霏,等.UPLC-MS/MS法同时测定牛奶中替米考星、地塞米松、氟苯尼考和氯霉素残留[J].中国畜牧兽医,2018,45(9):2645-2652.
[5] 农业农村部公告第250号《食品动物中禁止使用的药品及其他化合物清单》[Z].农业农村部公告第250号《食品动物中禁止使用的药品及其他化合物清单》[Z].2019
[6] GB 31650—2019 食品安全国家标准食品中兽药最大残留限量[S].
[7] 邹淼,冯静,陈曦,等.超高效液相色谱串联质谱法测定液态奶中氯霉素、甲砜霉素和氟苯尼考含量[J].食品安全质量检测学报,2020,11(20):7598-7602.
[8] GB/T 27404—2008《实验室质量控制规范食品理化检测》[S].
[9] SN/T1865—2016 出口动物源食品中氯霉素类残留量的检测方法[S].
[10] 李红权,孙良娟,伍志强,等.高效液相色谱串联质谱法同时测定饲料中氯霉素、甲砜霉素与氟甲砜霉素残留[J].分析测试学报,2012,31(11):1396-1400.
[11] 王浩,赵丽,杨红梅,等.液相色谱-串联质谱法测定牛奶中35 种四环素类、磺胺类、青霉素类、大环内酯类、氯霉素类抗生素残留[J].色谱,2015,33(9):995-1001.
[12] 赵飞,高广慧.超高效液相色谱-串联三重四级杆质谱测定蜂蜜中氯霉素的含量[J].山东化工,2016, 45(13):82-84.
[13] 张科明,梁飞燕,邓鸣,等. QuEChERS结合液相色谱-串联质谱法快速测定猪肉中多类兽药残留[J].色谱,2016,34(9):860-867.